34683-73-3Relevant articles and documents
Manganese-Mediated Direct Functionalization of Hantzsch Esters with Alkyl Iodides via an Aromatization-Dearomatization Strategy
Liu, Xian-Guan,Dong, Ci-Shuang,Li, Fei,Zhang, Bo
supporting information, p. 4002 - 4007 (2021/05/26)
We report, for the first time, manganese-mediated direct functionalization of the Hantzsch esters with readily accessible alkyl iodides through an aromatization-dearomatization strategy. Applying this protocol, a library of valuable 4-alkyl-1,4-dihydropyridines were facilely afforded in good yields. This simple and practical reaction proceeds under visible-light irradiation at room temperature and displays high functional-group compatibility. Additionally, the method is applicable for gram-scale synthesis and late-stage functionalization of complex molecules.
Preparation method of 1-chloro-6-iodohexane
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Paragraph 0011-0014, (2019/04/09)
The invention discloses a preparation method of 1-chloro-6-iodohexane. The preparation method comprises the steps of with 6-chloro-1-hexanol and p-toluene sulfochloride as the materials and benzene ortoluene as a solvent, reacting at (-5)-(5) DEG C for 2-5 hours under the effects of a phase transfer catalyst and an acid-binding agent so as to prepare 4-methylbenzenesulfonic acid-6-chlorohexyl ester, and carrying out reflux reaction on 4-methylbenzenesulfonic acid-6-chlorohexyl ester and sodium iodide for 0.5-3 hours, so as to prepare 1-chloro-6-iodohexane. The preparation method has the characteristics of easiness in operation, simplicity and convenience in after-treatment and relatively high yield.
Method for preparing hydrobromic acid teneligliptin
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, (2017/07/01)
The invention provides a method for preparing hydrobromic acid teneligliptin. The method includes steps of preparing L-hydroxyproline; mixing the L-hydroxyproline and sodium bicarbonate with each other to obtain mixtures, dissolving the mixtures in water, adding acetone into the water, dropping di-tert-butyl dicarbonate into the water, carrying out room-temperature reaction overnight and then treating reaction products to obtain t-butyloxycarboryl-N-hydroxyproline; preparing t-butyloxycarboryl-N-4-oxo-proline from the t-butyloxycarboryl-N-hydroxyproline; preparing (2S)-4-oxo-2-(3-thiazolidine carbonyl)-1-pyrrolidine carboxylic acid tert-butyl ester from the t-butyloxycarboryl-N-4-oxo-proline; preparing compounds III from compounds IV; preparing compounds II from the compounds III; preparing compounds 1-(3-methyl-1-phenyl-1H-pyrazole-5-base) piperazine from the compounds II; preparing intermediates I; preparing the hydrobromic acid teneligliptin from the intermediates I. The method has the advantages that the method is low in cost, and the cost of the method is only two-thirds of the cost of an existing method in the prior art; the yield of the hydrobromic acid teneligliptin is higher than 95%, and the purity of the hydrobromic acid teneligliptin is higher than 98%.